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当前位置: 首页 > 文章 > 婴幼儿配方奶粉中3-氯丙醇酯的GC-MS法测定及暴露危险分析 中国食物与营养 2016,22 (04) 15-19
Position: Home > Articles > Determination of 3-Chloro-1,2-propanediol(3-MCPD) Esters in Infant Formula Milk Powder by Using Gas Chromatography/Mass Spectrometry and Exposure Level Analysis Food and Nutrition in China 2016,22 (04) 15-19

婴幼儿配方奶粉中3-氯丙醇酯的GC-MS法测定及暴露危险分析

作  者：
许欣欣;陈慧玲;刘红河;康莉;毛丽莎
单  位：
深圳市疾病预防控制中心
关键词：
气相色谱—质谱联用;3-氯丙醇酯(3-MCPD酯);婴幼儿配方奶粉
摘  要：
目的:建立婴幼儿配方奶粉中3-氯丙醇酯的气相色谱—质谱联用(GC-MS)测定方法,并对部分市售婴幼儿配方奶粉中3-氯丙醇酯的含量进行调查。方法:用乙醚+石油醚(1∶1)提取奶粉样品中脂肪,以1 m L甲醇钠甲醇溶液(0.25 mol/L)将脂肪中的3-氯丙醇酯(3-MCPD酯)水解成3-氯丙醇(3-MCPD)并用硅藻土小柱净化后,经七氟丁酰基咪唑衍生,再用选择离子监测的气相色谱—质谱联用法测定,采用内标法定量。结果:3-MCPD酯在250~5 000μg/kg范围内线性良好(r>0.999),3个浓度水平下加标回收率为71.5%~99.6%,相对标准偏差为2.3%~6.0%。20份奶粉样品中,检出率65%,含量为0.26~0.97 mg/kg脂肪、0.042~0.22 mg/kg样品。不同阶段统计婴幼儿配方奶粉平均暴露量,一阶段3.32μg/(kg·bw)、二阶段2.42μg/(kg·bw)、三阶段2.72μg/(kg·bw)、四阶段0.23μg/(kg·bw)。结论:该方法灵敏度高、定量准确度,适合婴幼儿配方奶粉中3-氯丙醇酯的检测。
译  名：
Determination of 3-Chloro-1,2-propanediol(3-MCPD) Esters in Infant Formula Milk Powder by Using Gas Chromatography/Mass Spectrometry and Exposure Level Analysis
作  者：
XU Xin-xin;CHEN Hui-ling;LIU Hong-he;KANG Li;MAO Li-sha;Shenzhen Center for Disease Control and Prevention;
关键词：
GC-MS;;3-Chloro-1,2-propanediol(3-MCPD) esters;;infant formula milk powder
摘  要：
【Objective】To establish a determination method of 3-Chloro-1,2-propanediol( 3-MCPD) esters in infant formula milk powder by GC-MS,and investigate 3-MCPD esters residues in 20 kinds of infant formula milk powders from supermarket.【Method】Fat was extracted with Ether-Petroleum Ether( 1: 1) from infant formula milk powder,followed by hydrolyzed with 1. 0 m L sodium methylate solution( 0. 25 mol / L,inmethanol),and purified by matrix solid-supported liquid-liquid extraction. After being derivatized with heptafluorobutyrylimidazole( HFBI),3-MCPD esters were determined using GC-MS in SIM mode quantitativing by internal standard method.【Result】The method enjoyed a good linear and the detection limits were in the range of 250 ~ 5 000 μg / kg( r > 0. 999). The recoveries of the method were 71. 5% ~ 99. 6% and the relative standard derivation were 2. 3% ~ 6. 0%. In 20 kinds of infant formula milk powders,3-MCPD esters were detected at the range of 0. 26 ~ 0. 97 mg / kg fat and 0. 042 ~ 0. 22 mg / kg sample and the detection rates were 65%. Statistical average exposure levels at different stages of infant formula milk powders were 3. 32 μg /( kg·bw) for one stage,2. 42 μg /( kg·bw) for two stage,2. 72 μg /( kg·bw) for three stage and 0. 23 μg /( kg·bw) for four stage.【Conclusion】The method had higher sensitivity and accuracy,which could be applied to detect 3-Chloro-1,2-propanediol esters in infant formula milk powder.

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